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System and method for recovering PTA mother liquid and purifying and regenerating of catalyst
InactiveUS7314954B1Good purityImprove solubilityOrganic compound preparationChemical recyclingChemistryMother liquor
A system and a method for recovering PTA (purified terephthalic acid) mother liquid as well as purifying and regenerating catalyst, the system and the method is used mainly in manufacturing PTA wherein the mother liquid of the PTA generated by hydrogenation reaction is recovered by means of a PTA mother liquid recovering system to produce cobalt containing inorganic acid solution which is passed through a catalyst purifying / regenerating system and is electrolyzed with a cobalt purifying / regenerating system to produce metal cobalt which is then passed through an oxidized catalyst producing system to produce oxidized catalyst to be circulated for use in the process of manufacturing PTA.
Owner:MECHEMA CHEM INT CORP
Method for detecting Simotang preparation
ActiveCN102346177AEasy to separateGood symmetry factorComponent separationDigestive systemSilica gelAlkaloid
Owner:HUNAN HANSEN PHARMACEUTICAL CO LTD
Method for separating galanthamine from plant extract
The invention relates to a kind of effective constituent separation method in vegetation extract, especially the method of separating galantamine from vegetation extract containing amaryllidaceae alkaloid. The industrial art is as follows: make vegetation extract containing amaryllidaceae alkaloid have pretreatment; adsorb and elute with cation exchange resin; track and detect the elution flowing composition; make the flowing composition in galantamine have concentration and enrichment; after get virgin product of galantamine free alkali, make it have recrystallization with organic solvent; finally, the galantamine free alkali crystallization with about 99% purity can be acquired.
Owner:GUANGDONG TECHPOOL BIO-PHARMA CO LTD
Device and method for adopting electronic reaction beam for making ultrafine metal powder
The invention belongs to metal powder processing equipment and relates to a device and a method for adopting an electronic reaction beam for making ultrafine metal powder. According to the device, a crucible is arranged in an inner cavity of a vacuum evaporation chamber; a loading device and an electronic gun are arranged on a chamber wall; the vacuum evaporation chamber is communicated with the inner cavity of a vacuum receiving chamber through a pipeline with a vacuum valve; the inner cavities of the vacuum evaporation chamber and the vacuum receiving chamber are both connected with a vacuum pumping system controlled by a controller; a separator is arranged on an air outlet of the vacuum receiving chamber; the electronic gun is connected with a power controller; a circulating cooling device is arranged on each of the vacuum evaporation chamber and the vacuum receiving chamber. According to the method, a metal block is put into the crucible by the loading device, and after the metal block in the crucible is bombarded into gaseous metal by the electronic gun, the gaseous metal is collected by the vacuum receiving chamber and is cooled and separated by the separator, so that the ultrafine metal powder is achieved. The device and the method have the advantages of low energy consumption, high purity, wide application scope and suitability for the preparation of various ultrafine metal powder.
Owner:江永斌
Expressing Ompk antigen of outer-membrane protein of Vibrio Harveyi and application as constituent of bacterin
An expression of the Hawei's vibrio outer membrane protein antigen Ompk in colibacillus and the application of the recombinant outer membrane protein Ompk as the component of vaccine in preventing the vibrosis of sea fish are disclosed. Said recombinant protein is prepared through providing Hawei's vibrio EcGS020802 DNA as template, cloning the coding gene of Ompk by PCR method, recombining the gene in the prokaryotic expression carrier pBV220, efficient expression of the recombinant protein in colibacillus to become inclusion body, washing, modifying and renaturation. Its advantages are high purity and high output.
Owner:PEARL RIVER FISHERY RES INST CHINESE ACAD OF FISHERY SCI
Dimemorfan phosphate crystal form II and preparation method thereof, and pharmaceutical composition
ActiveCN102746227AGood pharmaceutical valueGood purityOrganic active ingredientsOrganic chemistryDrugDiffractometer
The invention provides a method for preparing dimemorfan phosphate crystal form II, which comprises the following steps: adding a crude dimemorfan phosphate product into methanol, heating under reflux to dissolve the crude dimemorfan phosphate product, cooling to precipitate crystals, filtering, and drying to obtain the solid dimemorfan phosphate crystal form II. The dimemorfan phosphate crystal form has the following X-diffractometer diagram characteristics; and in the X-ray powder diffractogram, interplanar distance d and Bragg angle 2theta represent the relative intensity relative to the percentage of the strongest line. The invention also provides a pharmaceutical composition containing the dimemorfan phosphate crystal form II as an active component and one or more proper auxiliary materials, such as tablets, capsules, granules, oral liquids, syrups, suspensoids and injections. The dimemorfan phosphate crystal form II has favorable pharmaceutical values, and has the characteristics of favorable purity, definite crystal form, excellent reproducibility and the like; and the dimemorfan phosphate crystal form II has valuable physiological activities in the field of preparations, and can be stored for a long time while remaining high stability.
Owner:杭州仟源保灵药业有限公司
Method for separating low-concentration naphthenic acid in wastewater and preparing naphthenic acid sample
ActiveCN102313659AGood purityPromote enrichmentPreparing sample for investigationChemistrySolubility
The invention discloses a method for separating low-concentration naphthenic acid in wastewater and preparing a naphthenic acid sample. The method comprises the following steps of: concentrating a dissolvable organic matter in the wastewater by using a reverse osmosis device; adjusting the pH value of reverse osmosis concentrated solution to be acid, and allowing the reverse osmosis concentrated solution to pass through an adsorption resin column to adsorb acid and neutral organic matters in the concentrated solution; backwashing the adsorption resin column by using alkali liquor; allowing the backwashing solution to pass through an H-type cation exchange resin column; putting the passed solution into a dialysis bag, and dialyzing in hydrofluoric acid solution for desilicification; evaporating in a rotating way, freeze-drying, and thus obtaining a small molecule naphthenic acid solid sample; backwashing precipitates on the H-type cation exchange resin column by using the alkali liquor; acidifying the backwashing solution, standing and collecting the precipitates; and filtering the precipitates, washing, centrifuging, freeze-drying, and thus obtaining a macromolecule naphthenic acid solid sample. By the method, the naphthenic acid can be separated from low-concentration naphthenic acid-containing wastewater, the recovery rate of the naphthenic acid is not less than 80 percent, and the prepared naphthenic acid samples have higher purity and are suitable for representation of various kinds of spectroscopy.
Owner:CHINA PETROLEUM & CHEM CORP +1
Process for the manufacture of montelukast sodium
Process for the manufacture of 1-[[[(1R)-1-[3-[(1E)-2-(7-chloro-2-quinolinyl)ethenyl]phenyl]-3-[2-(1-hydroxy-1-methylethyl)phenyl]propyl]thio]methyl]cyclopropane acetic acid, sodium salt [montelukast sodium (I)] consisting of: i. Converting methyl 1-(mercaptomethyl)-cyclopropaneacetate to a metal salt (X) using a metal hydroxide, ii. Subjecting the metal salt (X) to monometallation to provide a dimetallide (XI). iii. Converting a diol of formula (II) to a mesylate of formula (III) and reacting (III) in situ with (XI) affordin the metal salt of 1-[[[(1R)-1-[3-[(1E)-2-(7-chloro-2-quinolinyl)ethenyl]phenyl]-3-[2-(1-hydroxy-1-methylethyl)phenyl]propyl]thio]methyl]cyclopropane acetic acid. iv. Reacting the metal salt in-situ with a base and purifying to afford an amine salt (XII). v. Treating (XII) with a sodium base and precipitating out montelukast sodium (I).
Owner:GLADE ORGANICS PTE LTD
Method for preparing imipenem
The invention discloses a new method for preparing imipenem. The method comprises the following steps of: carrying out a Refortmasty reaction on an imipenem intermediate compound 4AA used as a starting material and an intermediate IX in the presence of a catalyst and obtaining an intermediate X through hydrolyzing; carrying out an N-H cabbeen insertion reaction on the intermediate X in the presence of a catalyst to obtain a double-ring parent nucleus III; in the presence of an organic base, phosphorylating to obtain an intermediate IV, directly reacting with cysteamine hydrochloride without separating, and then adding a proper solvent to obtain a solid solvent clathrate compound VI; directly carrying out condensation reaction on the solvent clathrate compound VI and imine benzyl oxide in the presence of base without removing the solvent to obtain an intermediate VII; and directly carrying out a catalytic hydrogenation reaction with the intermediate VII without separating to obtain a solution I containing the imipenem. The imipenem has a high content in the solution and can be crystallized by any known method in the field to obtain an imipenem-hydrate crystal.
Owner:SHENZHEN HAIBIN PHARMA +1
Unburned magnesia-carbon brick and preparation method thereof
The invention belongs to the technical field of high-duty refractory for electric furnace and converter linings and ladle linings and in particular relates to an unburned magnesia-carbon brick and a preparation method thereof. The unburned magnesia-carbon brick is characterized by comprising the following components in parts by weight: 80-90 parts of fused magnesite (more than or equal to 97% of MgO, the granularity of 0.1-5mm and the moisture content of less than or equal to 4%), 12-16 parts of graphite (more than or equal to 98% of C, the granularity of less than or equal to 400 meshes, and the moisture content of less than or equal to 0.15%), 0.5-1.5 parts of metal aluminum powder (more than or equal to 98% of Al and the granularity of less than or equal to 400 meshes), 1-3 parts of an aluminum magnesium alloy (more than or equal to 98% of Al+Mg and the granularity of less than or equal to 400 meshes), 0.2-0.8 part of boron carbide (more than or equal to 99% of BC4 and the granularity of 200-325 meshes), 1-2.5 parts of high temperature pitch (softening temperature of more than or equal to 150 DEG C, more than or equal to 50% of residual carbon and the granularity of 100-200 meshes), 0.2-0.5 part of a rare earth oxide (the granularity of 300-350 meshes), 3-5 parts of ceramic bond, 3-4 parts of a complex magnesium-aluminum cementing agent and 1-3 parts of water. The unburned magnesia-carbon brick disclosed by the invention has the advantages of simple and safe preparation method, low cost, no need of high-temperature firing, high density, high strength, high corrosion resistance, molten metal resistance, high oxidation resistance, energy conservation and emission reduction and the like.
Owner:孙光 +3
Method for purifying aesculin
InactiveCN109134562AHigh yieldGood puritySugar derivativesSugar derivatives preparationChemistryMother liquor
The invention discloses a method for purifying aesculin. The method comprises the following steps: drying and crushing Chinese ash roots; refluxing and extracting; combining extracts; abandoning material residues; concentrating the extract obtained in the step until no alcohol is left; placing the concentrate for crystallization; filtering and crystallizing; applying mother liquor to macroporous resin; respectively eluting with methanol with different alcohol degrees; collecting eluents with different alcohol degrees; concentrating the eluents; placing the concentrated eluent for crystallization; collecting all crystals together; adding new methanol for dissolving at 60 DEG C; filtering with a silica gel alumina column; collecting filtrate; concentrating and placing for crystallization; filtering crystals; drying the crystals and then adding purified water for dissolving at 95 DEG C for filtration; placing the filtrate for crystallization, wherein the crystals are aesculin and the content can reach 99%. Compared with the prior art, the method has advantages of high yield, good purity, short production period, simple process, safer operation and availability of high-purity aesculin.
Owner:宁县恒瑞康生物科技有限公司
Method for separating lycoramine from plant extract
The invention relates to a kind of effective constituent separation method in vegetation extract, especially the method of separating lycoramine from vegetation extract containing amaryllidaceae alkaloid. The industrial art is as follows: make vegetation extract containing amaryllidaceae alkaloid have pretreatment; adsorb and elute with cation exchange resin; track and detect the elution flowing composition; make the flowing composition in lycoramine have concentration and enrichment; after get virgin product of lycoramine free alkali, make it have recrystallization with organic solvent; finally, the lycoramine free alkali crystallization with about 99% purity can be acquired.
Owner:GUANGDONG TECHPOOL BIO-PHARMA CO LTD
Method for extracting gamma-livetin (IgY) from yolk
InactiveCN103570829AGood recoveryGood purityEgg immunoglobulinsPeptide preparation methodsYolkInorganic salts
Owner:王玉麒
Method for preparing octanohydroxamic acid
The invention discloses a method for preparing octanohydroxamic acid and belongs to the technical field of synthesis of cosmetic raw materials. The method is characterized by comprising the following steps: adding sodium hydroxide into a mixed system of hydroxylamine nitrate and methanol at the temperature of 0-10 DEG C under stirring conditions; adding methyl caprylate, carrying out a hydroxyl oximation reaction at the temperature of 30-60 DEG C for 2-6 hours, and filtering to remove sodium nitrate after the reaction is completed; distilling and recovering the methanol, cooling the reaction system to 0 DEG C, adding dilute nitric acid with the concentration of 5wt%, regulating the pH value to 3-4, separating out the solids, and filtering and drying so as to obtain octanohydroxamic acid; and separating the filtrate, recovering the oily matter, and performing water-phase concentration so as to obtain sodium nitrate solids, wherein the molar ratio of the methyl caprylate to hydroxylamine nitrate to sodium hydroxide is 1:(1-2):(2-3). According to the method disclosed by the invention, recycling of the solvent methanol is realized, a byproduct of sodium nitrate with relatively high economic value is obtained, and the method is mild in reaction conditions and favorable for industrial production.
Owner:禹城禹圳生物科技有限公司
Preparation method and application of organic framework supported CeO2/CuO electrocatalytic material
ActiveCN110586193AGood purityHigh repeatabilityOrganic-compounds/hydrides/coordination-complexes catalystsMetal/metal-oxides/metal-hydroxide catalystsChemistryMetal-organic framework
The invention belongs to the field of electrocatalytic overall water splitting, and particularly relates to a preparation method and application of a metal organic framework supported CeO2 / CuO electrocatalytic material. According to the method, the CeO2 / CuO electrocatalyst is prepared by using a coordination process, and the obtained electrocatalyst powder has high purity, better catalytic performance and high repeatability, and is easy to synthesize on a large scale; and the CeO2 / CuO composite electrocatalyst material exhibits excellent catalytic performance when applied to hydrogen evolutionand oxygen evolution reactions, achieves a current density of 10 mA*cm<-2> with overpotentials of 258 mV and 463 mV, respectively, and is a potential electrocatalytic overall water splitting catalyst.
Owner:东北大学秦皇岛分校
Overturn clearing-up type tartarian buckwheat conveying mechanism
InactiveCN106927196ALarge spreading areaGood synchronizationMagnetic separationLoading/unloadingPolygonum fagopyrumGear wheel
Owner:FUJIAN FLAVOR FOOD
Preparation method of 3-hydroxyl phthalic anhydride
The invention belongs to the technical field of organic synthesis and in particular relates to a preparation method of a key medical intermediate, 3-hydroxyl phthalic anhydride. The method comprises the following steps: with a compound I as a raw material, oxidizing the raw material to obtain 3-methoxyl phthalic acid; performing a reaction on 3-methoxyl phthalic acid to generate 3-hydroxyl phthalic acid; and performing dehydration and condensation on 3-hydroxyl phthalic acid to generate 3-hydroxyl phthalic anhydride. 3-hydroxyl phthalic anhydride prepared by the method provided by the invention is high in yield and good in purity. The method is free of special equipment demands, has mild conditions and is safe and environmental-friendly in an industrial process, and the process technology provided by the invention can be industrially performed.
Owner:JINAN XUANHONG BIOLOGICAL PHARMA CO LTD
Method for preparing key intermediate of Tofacitinib
InactiveCN109988174AGood purityOptimize the production processOrganic chemistryTofacitinibHigh selectivity
The invention provides a method for preparing a key intermediate (compound I) of Tofacitinib. The key intermediate of Tofacitinib is prepared through subjecting a compound II, which serves as a starting raw material, with a reaction with ammonium formate in the presence of a catalyst. The method for synthesizing the key intermediate of Tofacitinib-compound I, provided by the invention, has the aimof being applicable to industrial production and high-selectivity preparation. Through changing an experimental method, the generating of superhydrogenated impurities is avoided while operations canbe suitable for industrialization, so that the quality of the compound I can be controllable, and the quality of a finished product is better.
Owner:SHANDONG XINHUA PHARMA CO LTD
Preparation method of 2,2-difluoro-1,3-propanediol
ActiveCN107400040AHigh yieldGood purityPreparation by hydrogen halide split-offOrganic compound preparationDistillationPropanediol
The invention relates to the technical field of fluorine chemical engineering, in particular to a preparation method of 2,2-difluoro-1,3-propanediol. The preparation method is concretely characterized in that a sodium hydroxide water solution is used as a base solution; tetrabutylammonium bromide is added; 1,2-dichloro-1,1-difluoroethane is added; after reaction, the materials are introduced into a container containing carbon tetrachloride; dry ice cooling is performed to obtain 2-chloro-1,1-difluoroethylene; condensing and temperature reduction are performed; vacuumization is performed, so that a tetrachloromethane solution of the 2-chloro-1,1-difluoroethylene is sucked into a kettle; methyl alcohol, initiating agents, lauryl mercaptan and nanometer basic zinc carbonate are added; temperature rise reaction is performed; after the reaction is finished, reduced pressure distillation is performed to obtain 3-chloro-2,2-difluoro propyl alcohol; the 3-chloro-2,2-difluoro propyl alcohol is added into potassium hydroxide and N,N-dimethylformamide; after the reaction is finished, filtering is performed; filtering liquid is subjected to reduced pressure distillation to obtain the product. The preparation method has the advantages that the process is simple; the stability is good; the requirements on equipment are low; the preparation method is suitable for industrial production.
Owner:山东飞源新材料有限公司
Preparation method of high-cleanliness metal foil and preparation method of metal mask plate strip
PendingCN114433847AImprove cleanlinessLess investmentVacuum evaporation coatingSputtering coatingThin metalMetal foil
Owner:MAGIC STAR TECHNOLOGY (NINGBO) CO LTD
Hydrogen breathing machine with pressure detection function
The invention provides a hydrogen breathing machine with a pressure detection function. The hydrogen breathing machine comprises a water storage tank, a hydrogen generation device, a power supply device and a pressure detection system, wherein the water storage tank is used for storing water, and the hydrogen generation device is used for generating hydrogen and comprises an electrolytic chamber. A cathode plate, an anode plate and a permeable gas insulation film are arranged in the electrolytic chamber, the permeable gas insulation film is arranged between the cathode plate and the anode plate, the cathode plate and the anode plate enclose an electrolytic area, the permeable gas insulation film is used for dividing the electrolytic area into a hydrogen generation area and an oxygen generation area, the water storage tank is communicated with the oxygen generation area, the hydrogen generation area is used for enriching hydrogen and discharging the hydrogen out of the hydrogen breathing machine through an output pipeline, the power supply device is electrically connected with the anode plate and the cathode plate, and the pressure detection system is used for detecting the pressure of the hydrogen. On one hand, the hydrogen breathing machine with the pressure detection function can prepare high-purity hydrogen. On the other hand, the hydrogen breathing machine has a pressure display function, so that an operator can correctly adjust the hydrogen generation power and the on-off state of the hydrogen breathing machine.
Owner:SHENZHEN HYDROGEN HEALTHY WORLD HEALTH TECH HLDG CO LTD
Preparation method of carbosulfan
ActiveCN110950826ASolve the problem of long and cumbersome post-processingSolve technical problemsOrganic chemistryCarbofuranThermal insulation
Owner:湖南海利常德农药化工有限公司
Chemical semi-synthesis method of artemisinin
ActiveCN110590802AHigh yieldGood purityOrganic chemistry methodsChemical/physical/physico-chemical microreactorsDihydroartemisinic acidAcylation
The invention provides a chemical semi-synthesis method of artemisinin represented by a formula (VI) shown in the specification. The chemical semi-synthesis method comprises the following specific steps: (1) reacting dihydroartemisinic acid represented by a formula (I) shown in the specification with oxalyl chloride represented by a formula (II) shown in the specification to generate dihydroartemisinyl chloride represented by a formula (III) shown in the specification; (2) carrying out an acylation reaction on the dihydroartemisinyl chloride represented by the formula (III) and dihydroarteannuic acid represented by a formula (I) shown in the specification to generate dihydroarteannuic anhydride represented by a formula (IV) shown in the specification; and (3) carrying out a photooxidationreaction on the dihydroarteannuic anhydride represented by the formula (IV) by using a micro-channel reactor, and carrying out an oxidation rearrangement reaction to prepare the target product artemisinin represented by the formula (VI). Compared with the prior art, the method provided by the invention has the advantages of a high product yield, good purity of the product, a stable process, mild reaction conditions, easiness in industrial production and the like.
Owner:ZHEJIANG HISUN PHARMA CO LTD
Method for separating and purifying trimethyl benzene from C9 heavy aromatics
InactiveCN112457150AGood purityHigh yieldDistillation purification/separationCatalyst activation/preparationNitrogen atmosphereDistillation
The invention discloses a method for separating and purifying trimethyl benzene from C9 heavy aromatics. The method comprises the following steps: carrying out alkylation reaction on C9 heavy aromatics by using methanol as an alkylation reagent in a nitrogen atmosphere under the action of an alkylation catalyst; wherein the alkylation catalyst is a niobium oxide material loaded by a graphene / porous magnesium / aluminum metal oxide composite nano sheet; placing the alkylated solvent in a rectifying tower for reduced pressure distillation, collecting the (90-150) DEG C / 750mmHg fraction, and performing de-alkylation reaction on the collected fraction in a tubular furnace reactor in the presence of water vapor; putting the de-alkylated solvent into a cryogenic crystallizer, carrying out multi-stage cryogenic crystallization treatment, and then carrying out centrifugal treatment to obtain the trimethyl benzene crystal. The trimethyl benzene obtained by the method not only has high yield, butalso has high purity.
Owner:连云港鹏辰特种新材料有限公司
Method for growing zinc oxide monocrystalline under hydrothermal condition by utilizing mineralizer
ActiveCN102127802BFully developed</u><u>good purityPolycrystalline material growthFrom normal temperature solutionsZinc hydroxideSingle crystal
Owner:SHANDONG UNIV
Hydrogen breathing machine system with usage record analysis functions
InactiveCN107261272AGood purityImprove products and usage habitsRespiratorsCellsTime distributionPeripheral
The invention provides a hydrogen breathing machine system with usage record analysis functions. The hydrogen breathing machine system comprises a water storage tank, a hydrogen generation device, a power supply device and a host, wherein the water storage tank is used for storing water, the hydrogen generation device is used for generating hydrogen, the host is provided with a monitoring module and a wireless communication module, the monitoring module is used for recording use record of a use, the use record comprise use frequency, use time and use time distribution, and the wireless communication module is used for transmitting the use record to external devices. As the host of the hydrogen breathing machine can transmit the use record to the external devices such as a mobile phone and a server in real time, use regularity of the user is conveniently analyzed by a designer, a vendor and the user, products and use habits are conveniently improved, and normal use of the hydrogen breathing machine system is remotely stopped by a background. Further, the hydrogen breathing machine can be positioned in real time.
Owner:SHENZHEN HYDROGEN HEALTHY WORLD HEALTH TECH HLDG CO LTD
Periplaneta americana extract, odorless extraction method of periplaneta americana extract, anti-aging essence freeze-dried preparation containing periplaneta americana extract and preparation method thereof
PendingCN113520972AGood purityGood application prospectCosmetic preparationsToilet preparationsChemistryActivated carbon
The invention discloses an odorless extraction method of periplaneta americana extract, the method comprises the following steps: extracting at low temperature, concentrating and refrigerating to remove redundant grease, washing with a low-polarity organic solvent, adding activated carbon to adsorb sensitization substances and a heat source, finally filling into a gel column, and washing with water to remove substances capable of generating unpleasant odors, and finally obtaining the periplaneta americana extract without unpleasant odor. The whole extraction process is free of heating, active substances are not damaged, and the obtained extract or freeze-dried powder is good in purity and free of unpleasant odor and has good application prospects in the fields of health food and beauty and skin care. The invention also discloses an anti-aging essence freeze-dried preparation containing the periplaneta americana extract, which takes the periplaneta americana extract or freeze-dried powder as a main active substance and has the health-care functions of resisting inflammation, diminishing swelling, promoting skin healing, improving microcirculation, whitening, resisting aging and the like.
Owner:常州伟博海泰生物科技有限公司
Preparation method of 4AA diastereoisomer
PendingCN114685554AGood yieldGood purityGroup 4/14 element organic compoundsOrganic chemistry methodsAcetic acidIce water
Owner:WUHAN ZY PHARM CO LTD
Method of preparing titanium nitride-coated carbon black material through alkoxide hydrolysis
ActiveCN105670346AImprove thermal stabilityGood purityInorganic pigment treatmentChemistryIsopropyl alcohol
The invention provides a method of preparing a titanium nitride-coated carbon black material through alkoxide hydrolysis. The method includes the following steps: (1) adding methoxyl ethanol and tetraisopropyl titanate into anhydrous isopropyl alcohol and distilled water, mixing the components and performing a reflux reaction; (2) adding the carbon black, regulating the pH value to neutralization, and performing the reflux reaction for 2-4 h; (3) centrifugally filtering, washing and drying a product to obtain TiO2-coated carbon black particles; and (4) performing nitridation for 2-5 h by feeding ammonia gas at 800-1000 DEG C to prepare the titanium nitride-coated carbon black material, of which the surface is coated by the titanium nitride. In the method, firstly the carbon black is coated by the TiO2 to form the TiO2-coated carbon black material to improve chemical stability, and then the outer surface of the carbon black is coated by the titanium nitride, thereby greatly improving the thermal stabilities of the carbon black and the titanium nitride, so that the titanium nitride-coated carbon black material has excellent stability even at more than 1000 DEG C.
Owner:HEFEI GENIUS NEW MATERIALS
A preparation process of a clarithromycin impurity O or similar compounds
ActiveCN103232506AHigh product yieldGood puritySugar derivativesSugar derivatives preparationDimethyl sulfateKetone
A preparation process of a clarithromycin impurity O or similar compounds comprises: dissolving clarithromycin intermediates or oximation products (II) of B, C, D, E, F components as raw materials in a lower alcohol, a lower ketone or a halogenated hydrocarbon; and with methyl iodide, methyl bromide, or dimethyl sulfate as a methyl agent, and with the action of an acid-binding agent, subjecting to a methylation reaction at a temperature between 0-80 DEG C for 1 to 24 hours, after the reaction is completed, filtering, concentrating mother liquor under reduced pressure, and refining the residue in a mixed system of a lower alcohol with water or a mixed system of a lower ketone with water. The present invention provides a novel preparation process of the clarithromycin impurity O or similar compounds, the product yield is high, the purity is good, the crystallization is easy, and the purification is convenient.
Owner:HEC PHARM
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